The mesoporous Copper, nitrogen co-doped TiO 2 microspheres was prepared via solvothermal approach, followed by nitriding treatment under an ammonia gas flow. The crystalline structures of the as-prepared catalyst and the chemical compositions of Cu,N co-doped TiO 2 were determined using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) respectively. The photocatalytic activity of the as-prepared sample was investigated by monitoring the degradation of Rhodamine-B under visible light irradiation.Experimental results indicated that mesoporous Cu,N co-doped TiO 2 microspheres showed higher photocatalytic activity than Cu-TiO 2 microspheres and anatase TiO 2 under visible light irradiation. The higher photocatalytic activity of the mesoporous Cu,N co-doped TiO 2 microspheres sample could be attributed to the synergistic effects of large BET surface area, extended light absorption, efficient charge separation which was stabilized by the presence of oxygen vacancies. It was discovered that, valence states maintain stability after nitriding treatment. The sample synthesized from 0.1% molar quantity of Cu dopant, and nitrided at 400℃ for 30 min gave the highest photocatalytic activity.

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